Sladkov Vladimir, Fourest Blandine
CNRS, Institut de Physique Nucléaire, UMR 8608, Orsay, France.
J Chromatogr A. 2009 Mar 20;1216(12):2605-8. doi: 10.1016/j.chroma.2009.01.074. Epub 2009 Jan 29.
Separation and simultaneous determination of a number of organic acid anions (oxalate, mellitate, trimellitate and benzoate) and U(VI) with direct UV detection is developed for analysis of uranium carbide (UC) dissolution products by capillary zone electrophoresis (CZE). Reverse polarity mode is used. It is found that complex formation of U(VI) with carbonate, used as a carrier electrolyte, allows U(VI) to be determined, as negatively charged species, in a single run with organic acid anions. Some parameters such as pH value, composition of electrolyte and detection wavelength are optimized. Under the chosen conditions (carbonate buffer (ionic strength of 100 mM), pH 9.8, 0.15 mM tetradecyltrimethylammonium bromide (TTAB)) a complete separation is achieved. Calibration plots are linear in two ranges of concentration for U(VI) ( approximately 1 x 10(-5) to 1 x 10(-3)), mellitate and trimellitate ( approximately 5 x 10(-6) to 5 x 10(-4)), and about one range ( approximately 1 x 10(-4) to 5 x 10(-3)) for oxalate and benzoate. Accuracy of the procedure is checked by the "added-found" method in standard mixture solutions. Relative standard deviation is within the range of 2-10% and the recovery is in the range of 90-110%. This method is applied for the analysis of real UC dissolution samples.
建立了一种采用直接紫外检测法分离并同时测定多种有机酸阴离子（草酸盐、苯六羧酸盐、偏苯三羧酸盐和苯甲酸盐）以及U(VI)的方法，用于通过毛细管区带电泳（CZE）分析碳化铀（UC）的溶解产物。采用反相模式。研究发现，用作载体电解质的碳酸盐与U(VI)形成络合物，使得U(VI)能够作为带负电荷的物种与有机酸阴离子在一次进样中同时测定。对诸如pH值、电解质组成和检测波长等一些参数进行了优化。在选定的条件下（碳酸盐缓冲液（离子强度为100 mM），pH 9.8，0.15 mM十四烷基三甲基溴化铵（TTAB））实现了完全分离。U(VI)（约1×10⁻⁵至1×10⁻³）、苯六羧酸盐和偏苯三羧酸盐（约5×10⁻⁶至5×10⁻⁴）的校准曲线在两个浓度范围内呈线性，草酸盐和苯甲酸盐在约一个浓度范围（约1×10⁻⁴至5×10⁻³）内呈线性。通过在标准混合溶液中采用“加样-测定”法检查该方法的准确性。相对标准偏差在2 - 10%范围内，回收率在90 - 110%范围内。该方法应用于实际UC溶解样品的分析。
